Separation issues with 69ron non-toxic tek

[birdsarenotreal]

Hello fellow travelers.

A group of birds was signing about their experience with 69ron's D-Limonene Mescaline Extraction


The tek was followed as written; 100g of dried powdered cactus was mixed with 25g of calcium hydroxide in a french press.
300 ml of water was added to the mix. **the mix seemed a bit more watery than described in the tek.

300 ml of limonene was added and stirred until it seemed to incorporate into the mixture.

After a few hours, a small amount of limonene was observed to separate from the mixture.

The french press filter was pressed down but unable to separate the gunk from the solvent. Just lots of resistance.

The limonene layer was poured off to recover approximately 50-75 mL of solvent.




Is this normal to only recover 1/6 of the solvent initially added? It seems that an emulsion was possibly formed.

Could a hot water bath be used to help separate?

 

[birdsarenotreal]

Upon further reading of similar threads I would estimate that the water content in the mixture is too high.

The birds will add some additional cactus powder to dry and obtain a more desirable consistency.

 

[birdsarenotreal]

Additional 56g of cactus powder and 12g of calcium hydroxide were added and stirred into the mixture.

Immediately achieved much better separation and significant color change of the liquid portion. The color of the liquid portion is much darker now than in the previous mix.

 

[downwardsfromzero]

I'd also leave it to soak awhile so that the cactus has time to hydrate somewhat. Don't be surprised that the sludge/paste gobbles up most of the first portion of solvent. This should be compensated for by the subsequent pulls.

Microwaving would have been a convenient way to reduce the moisture content of the mix but once the limonene's in there you really don't want to be doing that (explosion risk!)

And liquid portion? Hopefully this is just limonene as you don't want any liquid water separating from the paste.

 

[birdsarenotreal]

I'd also leave it to soak awhile so that the cactus has time to hydrate somewhat. Don't be surprised that the sludge/paste gobbles up most of the first portion of solvent. This should be compensated for by the subsequent pulls.

Microwaving would have been a convenient way to reduce the moisture content of the mix but once the limonene's in there you really don't want to be doing that (explosion risk!)

And liquid portion? Hopefully this is just limonene as you don't want any liquid water separating from the paste.

Thank you!

Great point about the cactus hydrating a bit - there was a noticeable difference in texture after the powder/water mix sat for an hour or so.

As far as further reducing the moisture content without explosion risk, the birds had considered either a water bath or arranging a food dehydrator so it blows hot air into the french press.

Thankfully there seems to be an ideal water level at this point and limonene pulls have not pulled any water with them.

 

[Loveall]

The initial cactus paste consistency is very important. There are some complementary descriptions of what it should look like in the CIELO tek - FYI.

 

[birdsarenotreal]

The initial cactus paste consistency is very important. There are some complementary descriptions of what it should look like in the CIELO tek - FYI.

Good call - that is where the birds realized their mistake - those pictures are very helpful to determine the optimal consistency of paste.


Currently salting the limonene with vinegar and running into a bit of an emulsion. What do you think about adding some salt water to help break up the emulsion? The birds have been reading about salt's use in breaking emulsions but with the final material also in an aqueous layer, they are unsure how to remove the salt from the final vinegar mix.

 

[downwardsfromzero]

With salt you'll end up with salty product and attendant problems with measuring the dose. The only way to remove it would be another A/B cycle.

It's likely that particulates from the mix are causing the emulsion problem, and that adding further dry material to the mix after solvent was added has almost certainly exacerbated this. To that end, you could try filtering the liquid.

I think limonene is itself a bit of a pain. Ethyl acetate or butyl acetate are better. For future reference.

 

[shroombee]

I think limonene is itself a bit of a pain. Ethyl acetate or butyl acetate are better. For future reference.

Strongly agree. I've done many limonene tek extractions and many CIELO extractions. I highly recommend the OP look into CIELO.

 

[birdsarenotreal]

The milky emulsion layer seems to separate with additional time. The vinegar pulls are significantly less milky; waiting an additional 10 minutes or so before removing via pipette from the limonene/vinegar mixture.

to each of your points the cielo tek does look to be much more desirable - definitely avoids the messy acetate collection process.

in the local climate of the birds, many solvents are difficult to obtain easily but a journey to find ethyl acetate (aka MEK substitute) sounds like a worthwhile adventure.

Good thing they have ~3ft of TPQC cuttings that have been sitting in the dark for 3+ months. Time for more experiments!

 

[downwardsfromzero]

Ah, yes - waiting: the simple solution! Another idea might be to let the limonene settle before adding the vinegar. Decant after settling and maybe even filter, to be sure of removing maximum particulates.

[EA is used to clean certain types of 3D printing, and butyl acetate seems to have become increasingly popular of late as a substitute for a wide range of petroleum solvents.]

 

[birdsarenotreal]

Ah, yes - waiting: the simple solution! Another idea might be to let the limonene settle before adding the vinegar. Decant after settling and maybe even filter, to be sure of removing maximum particulates.

[EA is used to clean certain types of 3D printing, and butyl acetate seems to have become increasingly popular of late as a substitute for a wide range of petroleum solvents.]

Those plant teachers, always with the lessons!

EA should be easily obtainable online - perhaps there's a 3d printing supply store locally. The birds live in a liberal climate that is anti-VOC so stores like home depot have a severely limited selection compared to other climates.

The limonene has been filtered twice with coffee filters prior to salting with vinegar. Visible sediment was removed in each filter step.

The vinegar pulls are seemingly clearing up in the sep funnel so a 3rd filter step is likely to yield desirable results prior to evap.

If the birds are able to obtain EA prior to evaporating the vinegar, how might they incorporate a process whereas the crystals fall out of solution such as in the CIELO tek?
Could the vinegar be basified with NaOH, mescaline freebase pulled from the aqueous portion with EA and subsequently salted with citric acid?

 

[birdsarenotreal]

The birds evaporated some of the vinegar pulls and they were presented with what looks like calcium hydroxide contamination.

Any ideas on how to clean this up?

 

[birdsarenotreal]

imgonline-com-ua-dexif5n-FT0kd-YA2-Ix hosted at ImgBB

Picture of the material that was recovered from vinegar evaporation. Total yield over 5g and there is still more vinegar to be evaporated.

This suggests to me contamination of some sort.

They have NaOH, 99% IPA, Acetone, Fumaric acid and vinegar on hand to try and clean this up.

Possible solution:
1. Dissolve collected powder into 100mL water.
2. Add 50g of NaOH to basify solution and turn mescaline acetate into mescaline freebase
3. Add 100mL of limonene to dissolve mescaline freebase.
4. Pull non-polar limonene layer and reserve.
5. "wash" basified solution with another 100mL of limonene; separate and reserve limonene
6. Combine limonene fractions and add 100mL of vinegar. Mix well and allow to separate.
7. Pull vinegar fraction and evaporate.
8. Enjoy mescaline acetate free of calcium hydroxide.

 

[Loveall]

It may it work, and you may not have the chemicals, but I would make a paste with lime/water and your product, pull with ethyl acetate, rest in fridge, decant off water, and salt with citric acid.

It looks pretty good already. You can check the pH with pH paper and a drop of water on small sample to verify it is near neutral (it should be).

 

[doubledog]

2. Add 50g of NaOH to basify solution and turn mescaline acetate into mescaline freebase

You need much less NaOH to basify 100ml of water. 5 grams should be enough.

 

[birdsarenotreal]

It may it work, and you may not have the chemicals, but I would make a paste with lime/water and your product, pull with ethyl acetate, rest in fridge, decant off water, and salt with citric acid.

It looks pretty good already. You can check the pH with pH paper and a drop of water on small sample to verify it is near neutral (it should be).

This sounds like a great way to obtain some nice clean crystals - would you suggest a paste consistency similar to that advised in the CIELO tek (like a cookie dough texture)

And how much lime? 1g lime : 1g product?

You need much less NaOH to basify 100ml of water. 5 grams should be enough.

Good call thank you.